高锑铅中铅的测定  

Determination of lead in high antimony lead

作　　者：周姣连 谢磊 肖刘萍 ZHOU jiao-lian;XIE Lei;XIAO Liu-ping(ChenZhou Product and Commodity Quality Supervision and Inspection Institute,Chenzhou 423000,China;National Quality Supervision and Inspection Center of Precious Metal and Heavy Nonferrous Products(Hunan),Chenzhou 423000,China)

机构地区：[1]郴州市产商品质量监督检验所,湖南郴州423000 [2]国家有色贵重金属产品质量监督检验中心(湖南),湖南郴州423000

出　　处：《世界有色金属》2022年第2期93-95,共3页World Nonferrous Metals

基　　金：湖南省市场监督管理局科技计划项目(2020KJJH63)。

摘　　要：本文建立了硝酸-酒石酸混酸溶样-氢溴酸除锑-EDTA滴定测高锑铅中铅的分析方法。对溶样条件、酒石酸的加入量进行了研究,确立硝酸-酒石酸作为试样的溶样酸,且当样品量为2.0g时,其体积为50mL。考察了锑对铅测定的影响,锑的存在会使得铅的测定结果偏高,样品处理时必须除锑。干扰试验表明,按该实验方法共存元素不干扰铅的测定。将该实验方法应用于实际高锑铅样品中铅的测定,结果的相对标准偏差(RSD,n=8)为0.15%~0.20%,加标回收率在99%~101%之间。In this paper,an analytical method for determination of lead in high antimony lead by EDTA titration,that dissolved by nitric acid-tartaric acid and antimony removed by hydrobromic acid has been established.The solution conditions and the amount of tartaric acid were studied.Nitric acid-tartaric acid was determined as the solution acid of the sample,and when the sample amount was 2.0g,its volume was 50mL.The influence of antimony on the determination of lead was investigated.The existence of antimony would make the determination result of lead higher,and antimony must be removed during sample treatment.Interference test showed that coexisting elements did not interfere with the determination of lead.The relative standard deviation(RSD,n=8)of lead was 0.15%~0.20%,and the recoveries were 99%~101%.

关 键 词：高锑铅 硝酸-酒石酸混酸 氢溴酸除锑 铅的测定 

分 类 号：O657.31[理学—分析化学]